CsPbIBr2 Perovskite Solar Cell by Spray-Assisted Deposition - ACS

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Letter 2

CsPbIBr Perovskite Solar Cell by Spray Assisted Deposition Cho-Fai Jonathan Lau, Xiaofan Deng, Qingshan Ma, Jianghui Zheng, Jae Sung Yun, Martin A. Green, Shujuan Huang, and Anita Wing-Yi Ho-Baillie ACS Energy Lett., Just Accepted Manuscript • DOI: 10.1021/acsenergylett.6b00341 • Publication Date (Web): 17 Aug 2016 Downloaded from http://pubs.acs.org on August 18, 2016

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ACS Energy Letters

CsPbIBr2 Perovskite Solar Cell by Spray Assisted Deposition Cho Fai Jonathan Lau, Xiaofan Deng, Qingshan Ma, Jianghui Zheng, Jae S. Yun, Martin A. Green, Shujuan Huang, Anita W. Y. Ho-Baillie* Australian Centre for Advanced Photovoltaics, School of Photovoltaic and Renewable Energy Engineering, University of New South Wales (UNSW), Sydney 2052, Australia Supporting Information Placeholder

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ABSTRACT: In this work, an inorganic halide perovskite solar cell using spray-assisted solution processed CsPbIBr2 film is demonstrated. The process allows sequential solution process of CsPbIBr3 film overcoming the solubility problem of bromide ion in the precursor solution that would otherwise occur in a single-step solution process. The spraying of CsI in air is demonstrated to be successful and the annealing CsPbIBr2 film in air is also successful in producing CsPbIBr2 film with an optical bandgap of 2.05eV and is thermally stable at 300°C. The effects of substrate temperature during spraying and the annealing temperature on film quality and device performance are studied. The substrate temperature during spraying is found to be the most critical parameter. The best performing device fabricated using these conditions achieves a stabilised conversion efficiency of 6.3% with negligible hysteresis. Caesium metal halide perovskites remain viable alternatives to organic metal halide perovskites as the caesium containing perovskites can withstand higher temperature.

TOC GRAPHICS


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Organic-inorganic halide perovskites have emerged as competitive light harvesters due to their excellent optical absorption, good carrier mobility and lifetime.1 The power conversion efficiency (PCE) of organic-inorganic hybrid halide perovskite solar cells has improved rapidly from 9.7% to over 20% in a few years.2–6 These cells typically use organic cations such as methylammonium (MA) and formamidinium (FA). Although high PCE can be achieved, these cells are not thermally stable at high temperatures limiting module processing temperatures. One possible way to improve the thermal stability is to replace the organic cation with an inorganic cations such as caesium (Cs). Stoumpos et al. reported Cs containing perovskite has high mobility of holes (up to 320 cm2Vs-1) and electrons (up to 2300 cm2Vs-1) and estimated CsPbBr3 an electron mobility of ~1000 cm2Vs-1 and an electron lifetime of 2.5 µs.7,8 Kulbak et al. have demonstrated CsPbBr3 perovskite device with a PCE higher than 5%9,10 and Sutton et al. have reported CsPbI2Br cell with a maximum PCE at 9.8% and stabilized PCE at 5.6%.11 Ma et al. have also reported a hole transporting material (HTM) free CsPbIBr2 cell with a PCE at 4.7%.12 The best reported Cs perovskite device has a PCE of 6.5%.13 Perovskite films can be fabricated via solution process or physical deposition either in one-step or sequentially. Various deposition techniques include spin coating, 14,15 spraying 16,17 and thermal evaporation in ambient18,19 or in vacuum.12,20 Spraying, a widely used technique in industrial processes, has advantages over spin coating due to its ability to up-scale for large area cell or module manufacturing as well as its ability to coat conformally. Utilisation rate of material will also be higher for spraying compared to spin coating. Spray deposited perovskite solar cells have been demonstrated for organic-inorganic perovskite solar cells such as FA0.9Cs0.1PbI3 solar cell with a PCE at 14.2%.17 Spray deposition is yet to be demonstrated for solar cells using inorganic halide perovskites. In this work we report a two-step method of spray


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assisted solution processed CsPbIBr2 (with a bandgap of 2.05 eV) solar cells. Apart from the advantages of spraying mentioned above, this two-step method overcomes the issue faced by one step solution process of CsPbIBr2 perovskite film due to the poor solubility of the bromide ion in the precursor solution. The method can be scaled up when the PbBr2 is deposited by spraying instead of spin coating or physical deposition process such as evaporation. In this work, Au/Spiro-OMeTAD/CsPbIBr2/mp-TiO2/bl-TiO2/FTO/Glass solar devices are fabricated. For the deposition of the perovskite film, caesium iodide (CsI) is sprayed in air on a spin coated lead bromide film. A series of experiments investigating the effects of substrate temperature during spraying and post annealing temperature on the perovskite quality are conducted in this work. The optimised device produces a stabilised PCE of 6.3%. When measured under reverse scan, short-circuit current density (JSC) = 7.94 mA cm-2, open-circuit voltage (VOC) = 1121mV, fill factor (FF) = 70% and PCE=6.3%. When measured under forward scan, JSC = 7.84 mA cm-2, VOC = 1127mV, FF = 71.7%, and PCE = 6.2%. To investigate the effect of the substrate temperature during the spraying of CsI, the temperature of PbBr2/mp-TiO2/bl-TiO2/FTO/glass substrates was set at room temperature, 160°C, 350°C, during spraying in air. The samples were then annealed in air at 325°C for 10 min. Figure 1 (a) shows the X-ray diffraction (XRD) patterns of perovskite films prepared using different substrate temperatures. The main peaks at 14.82° , 21.05° and 29.94°correspond to the (100), (110), and (220) planes of the CsPbIBr2 perovskite orthorhombic phase.8,12 However, as substrate temperature increases (≥ 160 °C), CsI (27.5°)21 becomes prominent. An Energy dispersive Xray spectroscopy (EDS) measurement at 15 kV was carried out by a 17 µm line scan of the CsPbIBr2 films. Results are shown in Figures 1 (b)-(d) and the atomic ratios as a function substrate temperature are also summarized in a table in Figure 1. The results confirm that the


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perovskite film composition is of CsPbIBr2 when the film is deposited on a substrate kept at room temperature. As the substrate temperature increases to 350°C, the atomic ratios of Pb/Cs and Br/I decreases. This is consistent with the XRD results, suggesting that higher substrate temperature results in segregation of CsI.

Figure 1. (a) XRD patterns of the CsPbIBr2 films on /mp-TiO2/bl-TiO2/FTO glass substrate with varying substrate temperature during spraying. EDS (17µm line scan) spectra of CsPbIBr2 film deposited when substrate temperature is at (b) room temperature, (c) 160 °C, (d) 350 °C during spraying.


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Table 1. The atomic ratios of Pb/Cs and Br/I were calculated by averaging the atomic ratios of the 100 line-scanning points. Room Atomic Ratios

Temperature

160°C

350°C

Pb/Cs

1

1

0.4

Br/I

2

2

1

The effect of annealing temperature on the quality of the perovskite film was also examined. After the spraying of CsI on PbBr2/mp-TiO2/bl-TiO2/FTO glass substrates at room temperature in air, the samples were then annealed at 275°C or 300°C or 325°C or 350°C for 10 min in air. Good crystallinity can be achieved for all films annealed at temperature ranging from 275 to 350 °C as shown Figure 2 (a). The absorption coefficients (α) of the samples were calculated from their measured optical transmission (T) and reflection (R) spectra using α = ln((1 − R)/T). All of the absorption coefficients, see Figure S1 in supporting information, are above 5 × 10 cm-1 in the wavelength range of 575nm. The onset of the optical bandgap edge transition is round 600-615 nm (2.022.06 eV) which is similar to the CsPbIBr2 fabricated by dual source evaporation (2.05 eV).12 Figure 2 (b) shows the PL decay traces of sample with CsPbIBr2 annealed at different temperatures. Using bi-exponential decay function, the PL decay traces were fitted to determine the decay times of the fast (τ1) and slow (τ2) components which are summarized in a table in Figure 2(c). The presence of the fast component (τ1) in the PL decay indicates the presence of defect trapping and the slow component (τ2) corresponds to the radiative recombination time. A


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typical lifetime (τ2) above 11ns is found when the CsPbIBr2 film is annealed at temperatures in the range of 275 °C to 325 °C. This lifetime is comparable with that of CsPbIBr2 film (9.35 to 17.7 ns) reported in.12 Note, the lifetime dramatically drops when CsPbIBr2 film is annealed at 350 °C while the lifetime is longest when CsPbIBr2 film is annealed at 300 °C.

Figure 2. (a) XRD patterns and (b) PL decay traces and top view scanning electron microscopy (SEM) of the CsPbIBr2 films on mp-TiO2/bl-TiO2/FTO glass annealed at different temperatures (c) 275°C, (d) 300°C, (e) 325°C and (f) 350°C after spray-assisted deposition.


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Table 2. Typical lifetimes extracted from TCSPC for CsPbIBr2 with different annealing temperature. Lifetime

275°C

300°C

325°C

350°C

τ1

2.39

4.05

3.2

2.36

τ2

11.1

17.5

14.8

11.1

The morphology of the CsPbIBr2 films is also studied by the top view scanning electron microscopy (SEM) as shown in Figures 2 (c) to (f). Higher annealing temperature appears to result in a denser film as the size of pinholes reduces. Perovskite grains 500-1000nm in size are generally observed. To investigate the effects of substrate temperatures during spraying and annealing temperature on solar cell performance, Au/Spiro-OMeTAD/CsPbIBr2/mp-TiO2/bl-TiO2/FTO/Glass devices were fabricated under different conditions. Figure 3 (a) shows a cross sectional SEM image of a typical complete device where the bl-TiO2 is 45nm, the mp-TiO2/CsPbIBr2 layer is ~200 nm thick, the CsPbIBr2 over layer is ~160 nm thick and the spiro-OMeTAD is ~100 nm thick. The rest of Figure 3 shows that increasing substrate temperature causes drops in density–voltage (J-V) characteristics of the CsPbIBr2 device including JSC, VOC and also FF and PCE due to nonoptimum composition of the perovskite film as shown in Figure 1.


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Figure 3. (a) Cross-sectional SEM image a typical Au/Spiro-OMeTAD/CsPbIBr2/mp-TiO2/blTiO2/FTO device. (b) Current density–voltage (J-V) curves and (c) distribution (error bars are standard deviations) of PCE of Au/Spiro-OMeTAD/CsPbIBr2/mp-TiO2/bl-TiO2/FTO Glass cells fabricated using different substrate temperature during spray-assisted solution process of CsPbIBr2. Electrical characteristics of the best cell and an average cell in each category measured under reverse scan (open circuit to short circuit) are summarised in a table.


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Table 3. Photovoltaic Device Parameters of Au/Spiro-OMeTAD/CsPbIBr2/mp-TiO2/blTiO2/FTO device fabricated using different substrate temperature during spray-assisted solution process of CsPbIBr2. Substrate Temp. [°C]

JSC [mAcm-2]

VOC

FF

[mV]

[%]

Max. PCE [%]

Average PCE [%]

Standard deviation of PCE

RT

7.0

1079

72

5.4

4.8

0.56

160

5.3

931

58

2.9

2.6

0.32

350

3.9

965

58

2.2

1.0

0.77

Figure 4 shows that electrical performance of CsPbIBr2 cells when the substrate temperature is kept at room temperature during spray-assisted deposition while the annealing temperature is allowed to vary from 275°C to 350°C. Respectful performance (PCE>4.7%) can be achieved by cells when the CsPbIBr2 is annealed at temperatures in range of 275 °C to 325 °C. Planar as well as HTM-free devices were also fabricated at the optimal substrate (room temperature) and annealing (300°C) temperatures. Results are shown in Figure S2 in Supporting Information. Although the voltage of the planar device remains above 1V, fill factor and current suffer possibly due to the existence of pinholes in the CsPbIBr2. The HTM-free mesoporous device in this work is less efficient than the HTM-free planar device reported in 12 which could be due to the non-uniformity of the CsPbIBr2 film in this work. These findings suggest room for improvement for future devices using cesium perovskite films deposited using spray-assisted technique.


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Figure 4. (a) Distribution (error bars are standard deviations) of PCE and electrical characteristics of the Au/Spiro-OMeTAD/CsPbIBr2/mp-TiO2/bl-TiO2/ FTO glass devices measured under reverse scan when the CsPbIBr2 film is annealed at different temperatures, (b) current density–voltage (J-V) curves under reverse and forward scans (c) external quantum efficiency (EQE) and (d) stabilized PCE and maximum power point current density (JMPP) of the best performing CsPbIBr2 device.


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Table 4. Photovoltaic Device Parameters of Au/Spiro-OMeTAD/CsPbIBr2/mp-TiO2/blTiO2/FTO device fabricated scan when the CsPbIBr2 film is annealed at different temperatures. Annealing Temp. [°C]

JSC [mAcm-2]

VOC [mV]

FF [%]

Max. PCE [%]

Average PCE [%]

Standard deviation of PCE

275

7.0

1100

71

5.5

4.7

0.69

300

7.9

1121

70

6.3

5.7

0.47

325

7.0

1079

71

5.4

4.8

0.56

350

3.3

1166

70

2.7

2.3

0.54

Preliminary thermal stability test was performed on CsPbIBr2 films which involves heating at 300°C on a hot plate in a glove box for 1.5 hours. Results shown in Figure S3 in Supporting Information indicate no detectable phase change or the emergence of new impurity peaks or color change after the heat treatment indicating promising thermal stability of the CsPbIBr2 film. Finally, the PCE of the best performing cell measured under reverse scan at 30mV s −1 is 6.3% with a VOC of 1127mV, a JSC of 7.9 mA cm−2, and a fill factor of 72%. Under forward scan, PCE = 6.3%, JSC = 7.9 mA cm−2, VOC = 1121 mV, and FF = 71%. The external quantum efficiency (EQE) of the best device is presented in Figure 4 (c), together with the integrated current density as a function of wavelength. The integrated JSC is 7.03mAcm-1. The slightly lower integrated JSC from EQE is due to the lack of light soaking during EQE measurement. Light soaking that stabilizes the current density of the cell typically takes a few seconds. Stabilized PCEs was measured to be 6.3%. This is the highest stabilized efficiency achieved for an inorganic lead halide perovskite solar cell due to lower level of hysteresis. Our CsPbIBr2 cells have higher VOC compared with the VOC of the CsPbIBr2 cell fabricated via dual source evaporation which is


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959mV12. The short-circuit current of our cell can be further improved by increasing the thickness of CsPbIBr2 absorber to be beyond the current 160 nm. In summary, we have demonstrated an inorganic halide perovskite solar cell using spray-assisted solution processed CsPbIBr2 film. This allows sequential solution process of CsPbIBr2 film overcoming the solubility problem of bromide ion in the precursor solution that would otherwise occur in a single-step solution process. The spraying of CsI in air is demonstrated to be successful and the annealing CsPbIBr2 film in air is also successful in producing CsPbIBr2 film, thermally stable at 300°C, with an optical bandgap of 2.05eV. The effects of substrate temperature during spraying and the annealing temperature on film quality and device performance are studied. The substrate temperature during spraying is the most critical parameter as high substrate temperature will result in excess CsI in the film which has a detrimental effect on JSC, VOC and also FF. The optimal annealing condition of CsPbIBr2 is found to be 300°C for 10 minutes. The best performing device fabricated using these conditions achieves a stabilized conversion efficiency of 6.3% with negligible hysteresis. The grain size and morphology of the perovskite films are expected to be further improved for planar friendly or HTM-free device. The low hysteresis and the high stabilized power of the demonstrated spray-assisted deposited CsPbIBr2 cells mean cesium metal halide perovskites remain viable alternatives to organic metal halide perovskites as the cesium containing ones can withstand higher temperature. ASSOCIATED CONTENT Supporting Information Detailed experimental procedures, optical characterization, device performance of meso-porous vs planar devices and preliminary thermal stability results.


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AUTHOR INFORMATION Corresponding Author [email protected] Notes The authors declare no competing financial interests. ACKNOWLEDGMENT The Australian Centre for Advanced Photovoltaics (ACAP) encompasses the Australian-based activities of the Australia-US Institute for Advanced Photovoltaics (AUSIAPV) and is supported by the Australian Government through the Australian Renewable Energy Agency (ARENA). C. Lau is supported by the Australian Government and UNSW via Australian Postgraduate Award scholarship and Engineering Research Award respectively. Authors would like to thank Rui Sheng of UNSW for the cross sectional SEM imaging. We thank the Electron Microscopy Unit and the BioMedical Imaging Facility at UNSW for SEM and fluorescence imaging supports.


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REFERENCES (1) Green, M.A.; Ho-Baillie, A.; Snaith, H. J. The Emergence of Perovskite Solar Cells. Nat. Photonics 2014, 8, 506–514. (2) Eperon, G. E.; Stranks, S. D.; Menelaou, C.; Johnston, M. B.; Herz, L. M.; Snaith, H. J. Formamidinium Lead Trihalide: A Broadly Tunable Perovskite for Efficient Planar Heterojunction Solar Cells. Energy Environ. Sci. 2014, 7, 982. (3) Nazeeruddin, M. K.; Snaith, H.; Editors, G. Methylammonium Lead Triiodide Perovskite Solar Cells : A New Paradigm in Photovoltaics. MRS Bull. 2015, 40 , 641–645. (4) Kim, H.S.; Lee, C.R.; Im, J.-H.; Lee, K.B.; Moehl, T.; Marchioro, A.; Moon, S.J.; Humphry-Baker, R.; Yum, J.-H.; Moser, J. E.; et al. Lead Iodide Perovskite Sensitized All-Solid-State Submicron Thin Film Mesoscopic Solar Cell with Efficiency Exceeding 9%. Sci. Rep. 2012, 2, 1–7. (5) Kim, C.; Ryu, S.; Seo, J.; Seok, S. I. High-Performance Photovoltaic Perovskite Layers Fabricated through Intramolecular Exchange. Science Express 2015, 348, 1234–1237. (6) Saliba, M.; Matsui, T.; Seo, J.Y.; Domanski, K.; Correa-Baena, J.P.; Mohammad K., N.; Zakeeruddin, S. M.; Tress, W.; Abate, A.; Hagfeldt, A.; et al. Cesium-Containing Triple Cation Perovskite Solar Cells: Improved Stability, Reproducibility and High Efficiency. Energy Environ. Sci. 2016, 9, 1989–1997. (7) Stoumpos, C. C.; Malliakas, C. D.; Kanatzidis, M. G. Semiconducting Tin and Lead Iodide Perovskites with Organic Cations: Phase Transitions, High Mobilities, and nearInfrared Photoluminescent Properties. Inorg. Chem. 2013, 52, 9019–9038. (8) Stoumpos, C. C.; Malliakas, C. D.; Peters, J. a.; Liu, Z.; Sebastian, M.; Im, J.; Chasapis, T. C.; Wibowo, A. C.; Chung, D. Y.; Freeman, A. J.; et al. Crystal Growth of the Perovskite Semiconductor CsPbBr3 : A New Material for High-Energy Radiation Detection. Cryst. Growth Des. 2013, 13, 2722−2727.


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(9) Kulbak, M.; Cahen, D.; Hodes, G. How Important Is the Organic Part of Lead Halide Perovskite Photovoltaic Cells? Efficient CsPbBr3 Cells. J. Phys. Chem. Lett. 2015, 6, 2452–2456. (10) Kulbak, M.; Gupta, S.; Kedem, N.; Levine, I.; Bendikov, T.; Hodes, G.; Cahen, D. Cesium Enhances Long-Term Stability of Lead Bromide Perovskite-Based Solar Cells. J. Phys. Chem. Lett. 2016, 7, 167–172. (11) Sutton, R. J.; Eperon, G. E.; Miranda, L.; Parrott, E. S.; Kamino, B. a.; Patel, J. B.; Hörantner, M. T.; Johnston, M. B.; Haghighirad, A. A.; Moore, D. T.; et al. BandgapTunable Cesium Lead Halide Perovskites with High Thermal Stability for Efficient Solar Cells. Adv. Energy Mater. 2016, 6, 1–6. (12) Ma, Q.; Huang, S.; Wen, X.; Green, M. A.; Ho-Baillie, A. W. Y. Hole Transport Layer Free Inorganic CsPbIBr2 Perovskite Solar Cell by Dual Source Thermal Evaporation. Adv. Energy Mater. 2016, 6, 2–6. (13) Beal, R. E.; Slotcavage, D. J.; Leijtens, T.; Bowring, A. R.; Belisle, R. a; Nguyen, W. H.; Burkhard, G.; Hoke, E. T.; McGehee, M. D. Cesium Lead Halide Perovskites with Improved Stability for Tandem Solar Cells. J. Phys. Chem. Lett. 2016, 746–751. (14) Burschka, J.; Pellet, N.; Moon, S.-J.; Humphry-Baker, R.; Gao, P.; Nazeeruddin, M. K.; Grätzel, M. Sequential Deposition as a Route to High-Performance Perovskite-Sensitized Solar Cells. Nature 2013, 499, 316–319. (15) Kim, J.; Yun, J. S.; Wen, X.; Soufiani, A. M.; Lau, C. F. J.; Wilkinson, B.; Seidel, J.; Green, M. A.; Huang, S.; Ho-Baillie, A. W. Y. Nucleation and Growth Control of HC(NH2)2PbI3 for Planar Perovskite Solar Cell. J. Phys. Chem. C 2016, 120, 1126211267. (16) Barrows, A.; Pearson, A.; Kwak, C.; Dunbar, A.; Buckley, A.; Lidzey, D. Efficient Planar Heterojunction Mixed-Halide Perovskite Solar Cells Deposited via SprayDeposition. Energy Environ. Sci. 2014, 7, 1–7.


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(17) Xia, X.; Wu, W.; Li, H.; Zheng, B.; Xue, Y.; Xu, J.; Zhang, D.; Gao, C.; Liu, X. Spray Reaction Prepared FA1-x CsxPbI3 Solid Solution as a Light Harvester for Perovskite Solar Cells with Improved Humidity Stability †. RSC Adv. 2016, 6, 14792–14798. (18) Chen, Q.; Zhou, H.; Hong, Z.; Luo, S.; Duan, H.-S.; Wang, H.-H.; Liu, Y.; Li, G.; Yang, Y. Planar Heterojunction Perovskite Solar Cells via Vapor-Assisted Solution Process. J. Am. Chem. Soc. 2014, 136, 622–625. (19) Sheng, R.; Ho-Baillie, A.; Huang, S.; Chen, S.; Wen, X.; Hao, X.; Green, M. A. Methylammonium Lead Bromide Perovskite-Based Solar Cells by Vapor-Assisted Deposition. J. Phys. Chem. C 2015, 119, 3545–3549. (20) Liu, M.; Johnston, M. B.; Snaith, H. J. Efficient Planar Heterojunction Perovskite Solar Cells by Vapour Deposition. Nature 2013, 501, 395–398. (21) Triloki; Garg, P.; Rai, R.; Singh, B. K. Structural Characterization of as-Deposited Cesium Iodide Films Studied by X-Ray Diffraction and Transmission Electron Microscopy Techniques. Nucl. Instruments Methods Phys. Res. Sect. A Accel. Spectrometers, Detect. Assoc. Equip. 2014, 736, 128–134.


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